Mastic composition and flooring



. Patented Aug. 29, 1944 MASTIC COMPOSITION AND FLOORING Stuart P.Miller, Scarsdale, N. Y., assignor, by mesne assignments, to. AlliedChemical & Dye Corporation, a corporation of New York No Drawing.Application December 31, 1940,

Serial No. 372,677

9 Claims.

This invention relates to a bituminous mastic composition particularlysuitable for the formation of flooring and foot pavements, and toflooring and pavements formed of the new mastic composition.

Bituminous mastic compositions have been used in fioorings for manyyears. Heretofore known compositions for such use have comprisedasphalt, a mineral filler in the nature of mineral dust, and a mineralaggregate ordinarily comprising sand and gravel. Such compositions areapplied as flooring by heating the mixture of asphalt and mineralmaterial to a relatively high temperature at which the mixture isrelatively soft and plastic, and spreading the mixture on a surface tobe covered. Flooring employing these asphaltic compositions has sufferedfrom the disadvantage that where it is subjected to the action of waterit tends to absorb water and become'crumbly. Further, asphalt masticflooring is softened by the action of vegetable oils and petroleum oilsand vapors, to which it may be subjected in oil refineries or garages,so as to become unfit for use. It has also been found that such floorsexhibit an objectionable tendency to become soft at high temperatures,such as summer temperatures, to which they may be subjected.

It is an object of this invention to provide a new mastic flooringcomposition which is not substantially weakened or softened by water, bypetroleum oils and vapors; or by vegetable oils, and which by reason ofthese properties is particularly suitable for use to form a smooth,wearresistant flooring in factories, breweries,'garages, oilrefineries,etc., where the flooring is subjected to such agents.

It is a further object to provide a mastic composition which isapplicable at lower working temperatures than compositions heretoforeknown but which has improved resistance'to indentation athightemperatures and which is not readily cracked or shattered at lowtemperatures.

Other objects and advantages will appear from the following detaileddescription.

I have found that a mixture of a digestion pitch product such ascoal-digestion 1 pitch or an asphaltic pyrobitumen-digestion pitchproduct having a softening point (R. 8; B.) of 140 to 200 F., mineralfiller, substantially all of which passes a ZOO-mesh sieve, and mineralaggregate of controlled graduated sizes as hereinbelow explained and inregulated proportions hereinafter specifled, gives a mastic compositionwhich can be applied at lower temperatures than used for application ofasphalt mastic, which iscapable of use to form long-wearing flooring orother surface resistant to indentation and to the action of water,dilute acid, petroleum products and vegetable oils, and which is notsignificantly susceptible to temperatur changes normally encountered inthe use of which such flooring or other surfaces may be subjected, i. e.will not soften or bleed at summer temperatures, or shatter or crack atwinter temperatures.

The coal-digestion pitch may be produced by heating, while agitating,bituminous coal, for example, New York steam coal, Pittsburgh Seamcoking coal, or Ohio non-coking coal in intimate contact with tar,pitch, tar distillate or mixtures of these under specific temperatureconditions so that the coal is blended with the tar or tar products inwhich it is digested and the resultant mixture, when molten, behavessubstantially as a homogeneous fluid. The coal may be either a coking ora non-coking coal, The proportion of coal necessary will vary withtheparticular type of coal employed and also with the character of thepitch, tar or tar oil which is employed. I

The temperature to which the coal and tar or I pitch, which may be coaltar, water-gas tar, or

their distillationproducts, are heated varies with the particular typeof coal employed, but in general the temperature is around 300 0., sayfrom about 270 to 340 C.

The heating period in practice will vary, depending upon the quantity ofmaterial in the heatingvessel, the efilciency of the stirring apparatus,the amount of heating surface, etc. For small amounts of material, theperiod of heatingto raise the temperature to around 300 C. may be only acouple of hours or less; with larger gmounts in batch operation,especially where the agitation is less rapid, eight or ten hours, ormore, may be required in order to avoid overheating portions of thecharge.

Products especially adapted for the practice of this invention shouldcontain in general from 10% to 25%, up to 30%, of coal and should have asoftening point (R. 8: B.) of to 200 F., penetrations at 0 C. of notless than 1, at 25 C.

of 5 to 40, and at 461 C. of not more than '175.

The asphaltic pyrobitumen-digestion pitch product may be produced bydigesting an asphaltic pyrobitumen, having a fixed carbon content of atleast 50% and the chemical and physical properties listed below, withcoal tar, watergas tar, their pitches or distillate oils at atemperature of above about 240.,G., and preferably from 260 to 350 C.,for a sufilcient period that the asphaltic pyrobitumen is smoothlydispersed throughout the tar or tar products in which it is digested andthe resulting product when molten behaves substantially as a homogeneousfluid.

The chemical and physical properties of the asphaltic pyrobitumen whichis used togive the surprising result are: It is black incolor; has aspecific gravity of about 1.1 to about 1.25 at 77 F.; contains at least50% fixed carbon, and may contain from 50% to 90%; contains a smallamount of constituents soluble in carbon bisulfide, e. g. as little as2% and not more than about 6%; it is constituted almost entirely ofnon-mineral constituents insoluble in carbon bisulfide, e. g. as much as97% and not less than about 93%; is

.solid at. atmospheric temperatures; is substantially infusible; anddecrepitates on heating'in a flame.

An example of such asphaltic pyrobitumen is the material known asimpsonite, a large deposit of which occurs in La Flore County, Oklahoma.

The period of digestion maybe as long as two hours or more when thetemperature is below 260 C. and may be much shorter at highertemperatures. For example, in the digestion of impsonite at or above atemperature of 290 C.,

substantially complete digestion is attained within thirty minutes.Impsonite-digestion pitch products especially adapted for the productsof this invention should contain from about 5% to 50% of impsonite andshould have a softening point (R. 8: B.) of 140 to 200 F., andpenetrations at C. of not less than 1, at 25 C. of

.5 to 40, and at 46.1 C. of not more than 175.

The softening points and penetrations are determined in accordance withprocedure and using standard apparatus prescribed by the AmericanSociety for Testing Materials- Softening points referred to herein aredetermined bythe Ring and" Ball method. Penetrations are given .intenth-millimeters; in the caseof penetrations at 0 C., 200 grams areapplied for 60 seconds; for penetrations at C., 100 grams are appliedfor 5 seconds; and for penetrations at 46.1 C.,

mastic composition from 10% to 30% by weight passes a #40 sieve and isretained on a #200 sieve, from 10% to 40% by weight passes a #10 sieveand is retained on a #40 sieve, from 5% to 40% by weight passes a #4sieve-and is retained on a #10 sieve, and 0% to 25% by weight passes aone-half inch sieve and is retained on v a #4sieve. The mineral fillermay be slate dust,

limestone dust, silica, dust, clay, dolomite dust, pulverized slag,Portland cement, or similar fine mneral matter; the mineral aggregatemay be sand, crushed stone, slag, rock screenings, fine ravel, or othermineral material of suitable size and grading.

Proper control of the proportions of mineral particles of differentsizes has been found important in order' to-form a mastic composition.resistant to mechanical injury. In mastic products in which fro1n8% to17% of coal-digestion pitch or impsonite-digestion pitch is employed, Ihave found thatmineral particles of graduated sizes within the limits ofproportions given above combine smoothly with the digestion pitch andappear to interlock with each other to impart to the combination a highresistance to deformation.

The mastic.may be made on the site of the work, in either suitablemechanically operated heaters and mixers, or by manual stirring in openpans or kettles. The coal-digestion pitch or asphalticpyrobitumen-digestion pitch is heated to atemperature of from about 250to about 350" F. The mineral filler and mineral aggregate are heated toa temperature of from about 212 to 300 F. and then added to the melteddigestion pitch'. -The ingredients should be well mixed to effectuniform distribution of the particles. (During the mixing process, careshould be taken to avoid local overheating of the mixture, thetemperature of which should generally be maintained between 300 and 400F.) In an alternative procedure, the digestion pitch and a portion ofthe mineral, preferably all of the mineral filler and a quantity ofmineral aggregate passing a #10 sieve equal to the quantity of mineralfiller, may be heated and mixed elsewhere, molded in the form of cakes,and brought to the site of the work. The mastic cake are melted andcombined with additional digestion pitch and mineral aggregate as may benecessary to form the desired mastic composition.

A flooring or protective coating of digestion ,pitch mastic compositionis formed by applying the mastic composition to the work at atemperature of from about 300 to about 400 F. At such temperatures-themastic is a soft, spreadable mass which may be manipulated by suitabletools to form a layer of the'desired thickness. The mastic may beapplied in One or more layers to the surface to be covered to a uniformthick- 7 The mineral aggregate is consti- I tuted of graduated sizes sothat in the final pitch pounds of mineralaggreg'ate heated to a termness of from three-quarters to two inches.

tially cooling, to form a' compact mass having a smooth, wear-resistantsurface. The flooring or coating of mastic firmly adheres to the base orsurface to which it is applied, and is highly resistant to indentation.

The fOllOWing examples are illustrative of'experimental applications ofcoal-digestion pitch mastic flooring composition according to myinvention:

Example 1.325 pounds of coal-digestion pitch, having a softening point(R. & B.) of 173 F. and penetrations at 0 "C., 25. C. and-46.l C. of 7,wand 49 respectively, wereheated to a temperature of about 325 F. 200pounds of mineral filler heated to a temperature of about 250? F.,substantially all of which passed a #200 sieve, were added to the moltencoal-digestion and distributed therethrough.

perature of 250 F., composed of 365 pounds passing a #40 sieve andretained on a #200 sieve, 470 pounds passing a #10 sieve and retained ona #40 sieve, 920 pounds passing a #4 sieve and retained on a #l0'sieve,and 340 pounds Passing a one-half inch sieve and retained on a #4 sieve,were then incorporated in and uniformly distributed through the mixtureof coaldigestion pitch and mineral filler. This mastic mixture wasprepared on the site of the work which was a brewery, and the heatedmixture The top surface of ,the mastic is troweled, after parcomprising23% coal-digestionpitch and mineral matter consisting of equal parts ofmineral filler passing a #200 sieve and sand passing a #10 sieve wermelted with additional coal-digestion pitch at a temperature of about300 F., after which mineral aggregate at a temperature of 250 F. wasadded. The additional coal-digestion pitch and mineral aggregate wereadded in proportions to form a mastic having the following composition:

Per cent by weight Coal-digestion pitch, softening point (R. 8:

B.) 171 F., penetration at C., 9; penetration at 25 C., 21; Denetr ationat 46.1

The mastic composition described above was applied at a temperature ofabout 360 F. in a layer averaging about one inch thick to a section ofthe floor of an industrial laboratory, and the surface troweled to forma smooth flooring. This flooring was subjected to water, varioussolvents, oils of both tar and petroleum origin, and other chemicalswhich were spilled sistant material for'use in forming floorings orpavements in garages, oil refineries, laboratories, etc.

I While the invention has been described in its application to flooring,it is to be understood that the digestion pitch mastic composition maybe applied in other relationships such as covering railway structureswhere its mechanical strength and outstanding water-resisting qualitiesare desired. Still other applications of the mastic composition of theinvention are waterproofing of subways and lining of reservoirs, tanksand ducts.

thereon. The flooring was also subjected to heavy trafiic and impactfrom hand-trucks and heavy drums. After a-year of such wear, inspectionshowed no deterioration of the coal-diestion pitch mastic flooring.

Thus it is seen my digestion pitch mastic composition, having thefollowing analysis:

Per cent by weight Coal-digestion pitch or impsonite-digestion pitch,softening point (R. & B.) 140 to 200 F., penetration at 0 0., not lessthan 1; at 25 C., 5 to at 46.1 0., not more than 1'75 Mineral filler,substantially all passing forms a flooring which is resistant to wearand to indentation or deformation at the temperatures and otherconditions to which it may be subjected when in use. The composition isnot substantially weakened or softened by the action of water,petroleumproducts, vegetable oils and other reagents, so that "2 forms.jghly re- I claim:

1. A mastic composition consisting of from 8% to 17% by weight of adigestion pitch product obtained by heating a hydrocarbon-containingmineral substance with a member of the group consisting of coal tar,water gas tar and their oils and pitches at a temperatures above 240 C.and for a time such that the mixture is digested to form-a productwhich, when molten, behaves substantially as a homogeneous-fluid andhaving a softening point (R. & B.) of from 140 to 200 F., penetrationsat 0 C. of not less than 1, at 25 C. of from 5 to 40, and at 46.1 C. ofnot more than 1'75, mineral filler, substantially all of which passes a#200 sieve, in amount from 5% to 30% by, weight, and the remainder ofthe composition consisting substatnially entirely of not more than 30%mineral aggregate passing a #40 sieve and retained on a #200 sieve, notmore than 40% mineral aggregate passing a #10 sieve and retained pn a#40 sieve, not more than 40% mineral aggregate passing a #4 sieve andretained on a #10 sieve, not more than 2'5% to 17% by weight of adigestion pitch product obtained by heating a member of the groupconsisting of coal tar, water-gas tar. their oils and pitches with anasphaltic pyrobitumen containing not less than about 50% fixed carbon ata temperature above 240 (Land for a time such that the mixture isdigested to form a product which. when molten. behaves substantially asa homogeneous fluid, said digestion pitch product having a softeningpoint (R. 8: B.) of from 140 to 200 F.. penetrations at 0 C. of not lessthan 1, at 25 C. of from 5 to 40, and at 46.1 C. of not more than 175,mineral filler, substantially all of which passes a #200 sieve, inamount from 5% to 30% by weight, and the remainder of the compositionconsisting substantially entirely of not more than- 30% mineralaggregate passing a #40 sieve and retained on a. #200 sieve, not morethan 40% mineral aggregate passing a #10 sieve and retained on a #40sieve, not more than 40% mineral aggregate passing a #4 sieve andretained on a #10 sieve, not more than 25% mineral aggregate passing aone-half inch sieve and retained on a #4 sieve, and not more. than 15%asbestos fibers.

3. A mastic composition consisting of from 8% to 17% by weight of animpsonite-digestion pitch having a softening point (R. 8.: B.) of fromto 200 F., penetrations at 0 C. of not less than 1, at 25 C. of from 5to 40, and at 46.1

not more than 40% mineral aggregatepassiiig a #10 sieve and retained ona #40 sieve, not more than 40% mineral aggregate passing a #4 sieve andretained on a #10 sieve, not more than 25% mineral aggregate passing aone-half inch sieve and retained on a #4 sieve, and not more than 15%asbestos fibers.

4. A bituminous mastic composition consistin of from 8% to 17% by weightof coal-digestion pitch having a softening point (R. 8: B.) of from 140to 200 F., penetrations at C. of

not less than 1, at 25C. of 5 to 40, at 46.1 C.'

of not more than 175, mineral filler, substantially all of which passesa #200 sieve, in amount from 5% to 30% by weight, and the remainder ofthe composition consisting substantially entirely of not more than 30%mineral aggregate passing'a #40 sieve and retained on a #200 sieve, notmore than 40% mineral aggregate passing a sieve and retained on a #40sieve, not more than 40% ,mineral aggregate passing a #4 sieve andrefrom 10% to 30% passing a #40 sieve and retained on a #200 sieve, from10% to 40% passing a #10 sieve and retained on a #40 sieve, from to 40%passing a #4 sieve and retained on a #10 sieve, and from 0% to 25%passing a onehalf inch sieve and retained on a #4 sieve, the percentagesbeing based on the total weight of the mastic composition.

6. A flooring comprising a base and a wearresistant layer securedthereto, said layer beingcomposed of a mastic composition which isresistant to the action of water and petroleum products and alsoresistant to deformation at the temperatures encountered in use, andwhich 'comprises from 8% to 17% coal-digestion pitch having a softeningpoint (R. 81 B.) of 140 200 F., mineral particles mixed therewithcomprising, based on the total weight of the mastic composition, from 5%to 30% passing a #200 sieve, from 10% to 30% passing a #40 sieve andretained on a #200 sieve, from 10% to 40% passing a #10 sieve andretained on a #40 sieve, from 5% to 40% passing a #4 sieve and retainedon from 0% to asbestos fibers.

7. A mastic flooring composition resistant to the action ofwater andpetroleum products and also resistant to deformation at temperatures towhich it may be subjected, which comprises from 8% to 17% coal-digestionpitc having a softening point (R. & B.) of 140-200 F., mineral particlesmixed therewith comprising, based on the total weight of the masticcomposition,

-from.5% to 30% passing-a #200 sieve, from 10% to 30% passing a #40sieve and retained on a #200 sieve, from 10% to 40% passing a #10 sieveand retained on a #40 sieve, from 5% to 40% on a #4 sieve.

passing a #4 sieve and retained on a #10 sieve, and from 0% to 25%passing a one-half inch sieve and retained on a #4 sieve, and not morethan 15% asbestos fibers.

8. A mastic composition resistant to the action of water and petroleumproducts and also resistant to deformation at temperatures to which itmay be subjected, which comprises from 12% to 15% coal-digestion pitchhaving a softening point (R. & B.) of -200 F., mineral particles mixedtherewith comprising, based on the total weight of the masticcomposition, from 5% to 30% passing a #200 sieve, from 10% to 30%passing a #40 sieve and retained on a #200 sieve, from 10% to 40%passing a #10 sieve and retained on a #40 sieve, from 5% to 40% passinga #4 sieve and retained on a #10 sieve, and from 0% to 25% passing aone-half inch sieve and retained on a #4 sieve, and from 0% to 15%asbestos fibers.

9. A flooring comprising a base and a wearresistant' layer adheredthereto, said layer being.

the temperatures encountered in use, and which comprises from 12% to 15%fcoal-digestion pitch having a softening point (R. 8: B.) of 140-200 F.,and mineral particles mixed therewith comprising, based on the totalWeight of the mastic composition, from 5% to 30% passing a #200sieve,.from 10% to 30% passing a #40 sieve and retained on a #200 sieve,from 10% to 40% passing a #10 sieve and retained on a #40 sieve, from 5%to 40% passing a #4 sieve and retained on a #10 sieve, and from 0% to25% passing a one-half inch sieve and retained STUART P. MILLER.

